Graduates of PhD study program in the area of Inorganic Technology and Non-metallic Materials gain deep knowledge on scientific methods of research related to preparation of new types of non-metallic inorganic materials, with special focus on glass, ceramics, and surface modification of a broad range of various materials, including biomaterials. Graduates are able to solve problems related to inorganic technologies, development and characterization of new materials. They have special knowledge in the area of glass, inorganic binders, ceramic and refractory materials and inorganic additives. They have deep theoretical knowledge in the field of thermodynamics and kinetics and are capable of solving challenging engineering problems in technical practice. Graduates understand methods of studying structures as well as materials characteristics. They speak foreign languages, actively use computer and information systems, are able to work actively in teams, plan their own development within their research field and execute project management. Gained knowledge represents an excellent basis for obtaining a job either in academic or industrial research and development.

The project proposes to investigate the preparation of integrated self-healing systems for light metal alloys based on anodic, organic, hybrid and inorganic layers. These systems will be able to provide active behavior suppressing corrosion processes near defects combining different repairing mechanisms which will be progressively activated, to provide a prolonged life time.

Cr (VI) -based compounds represent the state of the art in corrosion protection of aluminum alloys in the aerospace field. The self-healing ability, present in the chromate conversion, is superior to any other protection system currently available, but European directives strongly limit the use of Cr (VI) for its health and environmental toxicity.

This project proposes to replace chromate conversion coatings by developing systems that combine different self-healing mechanisms in the same system, joining different layers that constitute a corrosion resistant architecture.

The project considers the development of anodic oxide layers for light alloys based on the incorporation of encapsulated corrosion inhibitors into the oxide layer and thus leading to self-healing ability. Then, a sol-gel coating will be deposited onto anodic films as an alternative sealing method to enhance the corrosion performance of these coatings. The infiltration of the anodic films using different sol-gel sols will be also considered.

In the sol-gel part, the development of novel inorganic films combining organic and/or inorganic inhibitors as salts (cerium or rare earth) will be considered. These inhibitors are activated by environmental parameters promoting the self-healing mechanisms effect; e.g. Glass-like CexOy coatings incorporating CexOy NPs. On the other hand, hybrid organic-inorganic coatings will be developed incorporating inhibitors with different release kinetics and activation mechanisms. In all cases, improve the density and adhesion to metals and paints and self-healing ability will be the principal goals.

The project involves the optimization of compositions and synthesis conditions together with the characterization of the integrated systems. The following general tasks will be carried out:

The alkali-activation is actually receiving a growing interest in the fields of ceramics. Usual alkali-activated materials, generally known as “geopolymers”, are produced through the reaction of an alumino-silicate raw material with an alkaline compound, which is typically a concentrated aqueous solution of alkali hydroxide or silicate. ‘Inorganic oligomers' (molecules with few Si4+ and Al3+ ions mutually bonded by bridging oxygens, with OH terminations) formed by dissolution of the raw materials undergo condensation reactions, with water release and formation of a gel, at low temperature (typically below 100 °C). Actual geopolymers yield a ‘zeolite-like' gel, consisting of a continuous, three-dimensional alumino-silicate network, generally possessing high chemical stability, so that, if inorganic wastes are included in the raw materials, pollutants may remain effectively trapped. The aim of the present investigation is the manufacturing of similar materials, from low temperature hardening, replacing most of mineral raw materials with inorganic waste, including recycled glassses. In case of condensation reaction not yielding a properly ‘zeolite-like' gel, the chemical stability could be enhanced by application of a thermal treatment (at moderate temperatures), promoting viscous flow of the glass fraction. In addition, the gelification will be exploited for the shaping, e.g. for the obtainment of foams (applied in thermal and acoustic insulation) by mechanical stirring of suspensions undergoing progressive hardening.

Silicone polymers are known as a fundamental class of preceramic polymers, yielding a remarkable amount of ceramic residue upon firing in air or inert atmosphere. Upon firing in air, silicones transform into amorphous silica, that may react with several oxides, dispersed in the starting polymer as reactive fillers (in form of oxide, hydroxides, carbonates etc.). The reaction may be exploited for the manufacturing of many types of silicate ceramics, especially in the form of highly porous bodies. In selected cases, a liquid phase formed by the melting of borate or phosphate fillers may catalyse the ionic interdiffusion and the synthesis of silicates; upon cooling, the liquid phase transforms into a glass phase, with the obtainment of new kind of glass-ceramics.

The aim of the present investigation is the manufacturing of highly porous glass-ceramics by application to silicone-based mixtures of additive manufacturing technologies, such as direct ink writing of silicone-based inks. In particular, reticulated 3D scaffolds, composed of bioactive glass-ceramic, will be a fundamental (but no the only) target, for applications in tissue engineering. Fine glass particles will be studied as well, as alternative reactive fillers.

4. A model for the relationships between structure and thermodynamics in phosphate glasses.

Phosphate glasses are a class of special materials with a broad interest in optical applications and since they possess large emission cross sections and low non-linear refractive indices they are ideal for their use as solid state matrices for the emission of laser radiation [1]. However, the use of glasses as laser hosts requires the production of generally large dimensions with a very high optical homogeneity and high quantum efficiencies, thus needing of very special processing conditions and a strict control of the glass composition. Additionally, the melting of phosphate glasses may also imply certain difficulties such as those regarding high volatility of their constituents, easiness of devitrification and rapid change of the viscosity with temperature due to their higher fragile character. The ability to choose the right composition as well as the adequate processing conditions for their preparation lies in the precise knowledge of the atomic structure and its influence on the glass properties.This project proposal will be carried out within the area of Optical Materials and its main objective will be to set up the fundamentals for a model based on the relationships between the thermodynamics and the structure of the phosphate melts and glasses. The core of the proposal will employ the theoretical methodology previously developed by the group at TnUAD for phosphate glasses that uses the Shakhmatkin and Vedishcheva thermodynamic model [2]. This approach uses structural data obtained through Nuclear Magnetic Resonance and Raman spectroscopies by which it was possible to calculate the Gibbs free energy of formation of the oxides in the glass composition [3]. The final aim of the project will be to obtain a model that based on the relationships between the structure and thermodynamics of the phosphate melts can be able to predict the glass forming ability and the main properties of the glasses.

This PhD work will be divided into two periods: the first, of two years, at the laboratories of CSIC for the preparation and study of the structure of the glasses; and a second of one year for the evaluation of the thermodynamic model at TnUAD.

The corrosion of the tableware glass (especially in dishwashing machines in the large gastronomy) and weathering during the storage as well as during the oversea transport is from the actual point of view one of the most important questions of the glass producers economic competition. The main aim of the dissertation is the study of composition – structure – property relationships of oxide glasses leading to the proposal of methodology enabling the prediction of glass resistance against corrosion and weathering. The methodology is established on the set of different glasses, with differences in chemical composition of the surface as well as in the bulk. The differences are justified with respect to thermodynamic modeling, surface tension measurement and surface composition analyses by progressive spectroscopic methods. Such obtained results should be put into correlation with glass corrosion and weathering process.

6. Photoluminescence properties of phosphors based on stoichiometric aluminates, silicates and alumina-silicates for applications in pc-WLEDs

The topic of a PhD. work is focused on the preparation of phosphors for applications in pc-WLEDs. Basic (un-doped) and doped (e.g. by Ce3+, Eu2+, Mn2+/Mn4+, or other RE and/or TM ions) systems as glasses (glass microspheres) and polycrystalline materials (as aluminates, silicates, luminosilicates) will be prepared and studied. The structure of un-doped glasses will be investigated by spectroscopic methods (MAS NMR, IR and Raman spectroscopy), then thermal properties (thermal analysis) and crystallization kinetics to characterise glass systems in details. Thereafter, RE and TM doped glasses and polycrystalline materials will be prepared and studied. The concentration of luminescence active ions will be optimised to achieve sufficient emission also in the red spectral region. The optical (UV-VIS-NIR) and photoluminescence properties will be studied in details: steady-state PL, decay curves (TCSPC), effect of temperature on PL properties. The special attention will be placed on: relation of emission properties (after excitation by blue/NUV light) vs. structure and morphology of materials, concentration of RE and TM ions, effect of alkaline earth ions on emission properties of material.

7. Preparation and luminescence study of long lasting phosphors with melilite structure

The topic of a PhD. work is focused on the preparation of long lasting phosphors with light emission up to several hours after sample irradiation exposure to UV light. Doped (e.g. by Eu2+, Mn2+, Dy3+, or other RE and/or TM ions) aluminosilicate systems will be prepared in the form of glass (glass microspheres) and polycrystalline materials of melilite structure (e.g. with ackermanite (Ca2MgSi2O7) and gehlenite composition (Ca2Al2SiO7)). The prepared materials will be characterised from the point of morphology (e.g. optical microscopy, SEM), phase composition (XRD), structure (MAS NMR, IR and Raman spectroscopy), thermal properties (thermal analysis) and spectral properties (UV-VIS-NIR, fluorescence spectroscopy, EPR spectroscopy). The effect of glass vs. crystalline matrix, type of alkaline earth ions in glass and polycrystalline, and RE/TM concentration on emission intensity and afterglow decay time will be studied in detail. The mechanism responsible for afterglow emission will be proposed for studied materials; the known afterglow mechanisms will be assessed critically.

8. Structure and properties of hybrid inorganic-organic coatings based on nanomaterials.

The field of nanomaterials is the one of the crucial research field in the present days and the attention is focused on hybrid materials. Sophisticated possibility for preparation of hybrid inorganic-organic materials is connected with the assembling or the dispersion of well-defined nanobuilding blocks (NBB) which consists of perfectly calibrated preformed objects that keep their integrity in the final material.

The aim of the project is the investigation of the relationship between composition, structure and properties in relation to the hybrid inorganic-organic coatings based on nanomaterials , prepared in the system (EtO)3SiR–(EtO)4Si–IPA–cat–H2O, where (EtO)3SiR is trietoxyalkylsilane while R will be –CH2–(CH2)n–CH3, –CH2–(CH2)n–NH2 or –CH2–(CH2)n–CH=CH2, according to the required surface properties; (EtO)4Si is tetraetoxysilane; IPA is isopropyl alcohol and „cat“ is acidic or base catalyst of hydrolysis.

The methodology relating to composition – structure – properties relationship will be based on the creations of models and making them more precise for the specific cases. In the process of investigation, the designed experiments will be performed in order to preserve precise and detailed description of relationship between composition, structure and properties. The creation of the models describing the composition – structure – properties relationship will be based on utilisation of mathematical-statistical approaches involving regression analysis.

9. A multi-analytical approach for the optimal efficiency of historical glass conservation

The main target of the project is the development of innovative methodologies to test the effectiveness of historical glass conservation procedures and products. Historical glass, either of archaeological and artistic interest or architectural, needs tailor-made conservative protocols that need to be tested and verified. The project aims at evaluating the efficacy of the protocol in different operating conditions and in the medium and long-time protection. Tests will be made on commercial cleaning, adhesive, consolidating and protective products by testing chemico-physical, mechanical and aesthetic properties. If appropriate (i.e. for architectural glass) accelerated ageing tests will be used in investigations on the degradation behaviour of outdoor heritage materials. Real samples and artificial substrates produced on the basis of the most representative recipes used in the production of colourless and coloured/opaque glass will be subject to multi-analytical protocols.

10. Incorporation of fibrous/particulate bioglasses in hydrogels and other soft matrices for soft tissue engineering approaches

The material for the human body requires besides demand of its bioactivity and overall surface compatibility also suitable microstructure, reproducible porosity and mechanical properties also reffered to as structural compatibility. The adjustment of this compatibility on microscopic and macroscopic level are necessary for the optimal transport of nutrients, migration of cells to the implant-tissue interface, their proliferation and effective connection to the body tissue1.Incorporation of fibrous/particulate bioglasses in hydrogels and other soft matrices is the way how to achieve the requested properties of biomaterials intended for soft tissue engineering approaches, in order to increase the bioactivity and promote cell attachment in these materials2. The aim of the dissertation project will be therefore aimed at the development of new types of bioglass/hydrogel/biopolymer composites aimed at the use in soft tissue replacement. Particular interest will be paid to optimising the bioglass/soft matrix interfaces, porosity, and mechanical properties of the composites. Selected materials will be the tested with respect to their bioactivity in-vitro, with extension to in vivo tests in the most promising candidates.

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